RESUMO
Aflatoxins (AFs), an important category of pollutants, are formed in many foods and adversely affect human health. Therefore, their determination is critical to ensuring human food health. An efficient dispersive solid-phase microextraction technique was developed as a simple and straightforward sample preparation technique for determination of four aflatoxins using a high-performance liquid chromatography (HPLC) fluorescence detector. A novel efficient, green sorbent for extracting AFs was synthesized based on hydrothermal and chemical strategies. The amounts of three sorbent components were optimized using a mixture design (simplex lattice design), including 14 experiments. The optimal amount of amino-bimetallic Fe/Ni-MIL-53 nanospheres, chitosan, and magnetic Fe3O4 nanoparticles as sorbent components was 0.87, 0.67, and 0.47 g, respectively. Also, various factors affecting the process of AF determination were studied and optimized in two successive experimental designs, including the definitive screening design and the Box-Behnken design. Under optimal conditions, the linear ranges for measuring aflatoxin B1, aflatoxin B2, aflatoxin G1, and aflatoxin G2 were 0.05-82.6, 0.07-86.4, 0.08-85.7, and 0.07-89.5 ng mL-1, respectively. The relative standard deviations under inter-day and intra-day conditions for measuring AFs at three analyte concentrations were determined in triplicate analysis and were in the ranges of 3.7-4.6% and 4.9-6.1% for water sample analysis, respectively. The qualitative detection limits for determining AFs were between 0.01 and 0.05 ng mL-1. The pre-concentration factor of the method for measuring AFs ranged from 739.7 to 802.1. The proposed method was used for determining AFs in several real samples, including herbal distillate, black tea, corn, and real water samples. The relative recovery and standard deviation were 87.8-97.8% and 4.10-6.82%, respectively.
RESUMO
This paper introduces a novel and minimized sample preparation technique based on hollow fiber-protected liquid-phase microextraction that can be used in joint with gas chromatography-mass spectrometry (GC-MS) detection to extract three organochlorine pesticides-Endrin, Chlordane, and Dieldrin-from rice samples. To that end, a single-walled carbon nanotube (SWCNT) and a proper ionic liquid (IL) were ultrasonically dispersed and injected into the lumen of hollow fiber as the extraction phase for preconcentrating and extracting the target analytes from the rice samples. The effects of the type of nanoparticles, ILs, and desorption solvent on the efficiency of extracting the analytes were investigated based on the one-factor-at-a-time (OFAT) approach. In addition, other parameters influencing the extraction procedure were optimized using an experimental design that decreased the number of experiments, reagent consumption, and costs. Under optimized conditions, the limits of detection and quantification in determining mentioned pesticides varied between 0.019-0.029 and 0.064-0.098 ng mL-1, respectively. The calibration graphs to measure Endrin, Chlordane, and Dieldrin were linear over the concentration range of 0.064-13.2, 0.098-16.7, and 0.092-11.4 ng mL-1, respectively. The relative standard deviations for inter-day and intra-day analysis were below 7.06 and 4.75% for the triplicate determination of three organochlorine pesticides. Besides, the relative recoveries and standard deviations of Endrin, Chlordane, and Dieldrin for analyzing several Iranian rice samples were between 86.0-92.9% and 4.5-5.8%, respectively. The results were compared with other similar works in literature, proving that the proposed method is efficient and useful for routine monitoring of organochlorine compounds in food samples.